Dyes and process of making same



isms

FICE.

nosm'r AIR-NOT, 01* BUsnEY, ENGLAND.

nvns Am) rnocnss or MAKING SAME.

No Drawing.

To all whom it may concern:

Be it known that I, Roenn'r Armor, a citizen of the Czechoslovak Republic, residing at Bushey, Herts, England, have invented certain new and useful Improvements in' Dyes and Processes of Makin Same, of which the following is a speci cation.

Ex eriments have shown thatby distilling a ietic acid or resins, which are its more or less impure state, with burnt lime or sodalime there will be obtained phenol-like products which may constitute the starting materials for the making of dyestuffs.

The object of my invention resides in the feature of introducing chromophore or auxochrome groups, which I deslgnate nerically as chromogenetic, or groups 0 both kinds, into the bodies obtained by distilling resins with burnt lime or soda-lime and either to employ the resulting bodies per so as dyestufl's or to couple them with such bodies as are already employed for the making of azo-dyes. By these means a considerable number of new dyestufi's yielding the most diverging variety'of tints will be ob: tained.

Example.

50 parts by weight of finely powdered colophony are well mixed with equal arts of fresh] burnt, finely ground lime, t e mixture t en heated in a retort yields from 150 to 300, 25 parts of a clear nearly colourless oil, with greenish fluorescence. This is introduced, while bein mixture com osed o 15 parts by weight of nitric acid 1.45) and 25 parts by wei ht of concentrated sulphuric acid. A s'o id nitro-compound is separated, which is reduced and diazotized 1n the following manner:

10 parts by weight of the powdered nitro compound are dlssolved in 30 parts by wei ht of a hot 10% solution ofcaustic soda, while a concentrated solution of sodium-hydrosulphite is added to the boiling solution. The mixture is strongly boiled in a vessel provided with a reflux cooler for the s ace of an hour, whereu on dilute hydroch oric acid is gradually a ded to the continuously boiling solution until the sulphurous acid has been completely expelled. It is advisable to add w1th the hydrochloric acid also some acetic acid to keep the amino-phenol stirred,.into a cooled Application filed August 81, 1921. Serial No. 497,358.

resin in solution. Hereupon the solution is cooled with ice and diazotized. The-diazo compound couples fon instance with R salt (sodium salt of 2 naphtol, 3-6 disulphonic acid) wine'red, with G salt (2 naphtol, 6-8 disulphonic acid) brownish red, with chromotrope acid (1, 8 oxy, 4-5 disulphonic acid) violet, with H acid (1 amino 8 oxy 3, 6 disulphonic acid) violet blue. To obtain a black dye the diazo compound is introduced, while bein stirred, into the solution of a predetermlned quantity of a naphthylamine in acetic acid. Afterbeing allowed to stand overnight, one separates out the black precipitate,which is repeatedly washed with hot dilute hydrochloric acid and thereupon dissolved in a hot 10% soda solution.

. combination with H acid.

The dyeing operations are performed by putting the wool into the dye bath. at a, temperature of 50 whereupon 2% of sulphuric acid is gradually added and the wool allowed to remain in the dye bath for the space of an hour at 90. The vat will only be partially discolored.

From the residue in the retort (i. e:, residue obtainedby heatin the rosin and lime there may be isolated ot er phenol-like pro ucts either by extraction with alcohol or-b boiling with acids. These products will 8851 1 dissolve in soda and may be coupled with iazo-compounds.

What I claim is: I

1. The process which comprises distilling a resin with lime, nitratingthe henol-like body formed thereby and reduclng the resulting nitro compound to an amino compound.

2. The process which comprises distilling a resin w1th lime, nitrating the phenol-like body formed thereby, redilcing the resultin nitro compound to an amino compound an diazotizing the resulting amino compound.

3. The rocess which comprises distilling a resin w1th lime, nitrating the phenol-like v The dark -orange coloured solution thereby produced body formed thereby, reducing'the resulting nitro compound to an amino compound, diazotizing the resulting amino compound and coupling the resulting diazo compound with another compound to form an azo dye.

4. The process'which comprises distilling 21 resin with lime, uitrating the phenol-like. body formed thereby, reducing the nitrocompound to an amino compound, and coupling the same with another compound to form an azo dye, one of said compounds being diazotized before the coupling operation.

5. The process which comprises distilling a resin with lime, nitrating the phenol-like body formed thereby and introducing thereinto a chromophorous group.

6. The rocess which comprises distilling a resin with lime, nitrating the phenol-like body formed thereby, and introducing thereinto chromophorous and auxochromous groups.

7. The process which comprises distilling a resin with lime, nitrating the phenol-like body formed thereby, and introducingthereinto a chromogenetic group.

8. The process WhlCll comprises distilling a resin with lime, nitrating the phenollike body formed thereby and introducing thereinto chromogenetic groups.

9. An azo dye comprising a coupling roduct of the amino derivative of a pheno -like body formed by distilling resin with an alkali, and another amino aromatic body, one of said compounds being diazotized before the coupling operation.

10. An azo dye comprisin a coupling product of an amino-aromatic iody with the diazo amino derivative of the phenol-like product from the distillation of resin.

In testimony whereof I have hereunto set my hand in presenceof two subscribing witnesses.

ROBERT ARNOT. Witnesses:

DAVID BLEEDLUP, DAISY JEWELL. 

